Production of spherical ceramic powders

• US 5,064,783 A
• Filed: 05/08/1990
• Issued: 11/12/1991
• Est. Priority Date: 07/31/1989
• Status: Expired due to Term

• Current Assignee: Bodycote Ortech Inc., Ortech Corporation (Bodycote PLC)
• Original Assignee: Ortec International, Inc.
• Inventors: Luckevich, Lydia M.
• Primary Examiner(s): Dixon, Jr., William R.
• Assistant Examiner(s): GALLO, CHRISTOPHER
• Application Number:
  US07/520,769
• Time in Patent Office: 553 Days
• Field of Search: 501/12, 502/8, 423/625, 423/628
• US Class Current: 501/12
• CPC Class Codes: C01B 13/32 by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
• CPC Class Codes: C01B 33/26 Aluminium-containing silicates , i.e. silico-aluminates
• CPC Class Codes: C01F 7/162 Magnesium aluminates
• CPC Class Codes: C01G 25/00 Compounds of zirconium
• CPC Class Codes: C01P 2004/32 Spheres
• CPC Class Codes: C04B 35/10 based on aluminium oxide
• CPC Class Codes: C04B 35/119 with zirconium oxide
• CPC Class Codes: C04B 35/624 Sol-gel processing
• CPC Class Codes: C04B 38/0045 by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
• CPC Class Codes: C04B 38/009 Porous or hollow ceramic granular materials, e.g. microballoons C04B18/027, C04B20/002 take precedence

Abstract

A sol-gel method is employed to produce ceramic oxide spheres from precursors thereto. An alkanol of the sol precursor(s) is introduced to an immiscible hydrophilic liquid phase to cause spheroidizing of the sol. Moisture, which initially may be present in the immiscible liquid or may subsequently be added, is employed to effect hydrolysis of the precursor to oxide form. The ceramic oxide spheres are recovered from the liquid phase and calcined to their final form.

Claims

1. A method of producing ceramic spheres suitable for calcination to ceramic powders, which comprises:

contacting an anhydrous alkanol sol of at least one ceramic oxide precursor with liquid with which said sol is immiscible to form spheres of said sol in said immiscible liquid, and

hydrolyzing said ceramic oxide precursor in said spheres to form ceramic oxide spheres.

2. The method of claim 1 wherein said spheroidizing step and hydrolysis step are effected sequentially.

3. The method of claim 1 wherein said spheroidizing step and hydrolysis step are effected simultaneously.

4. The method of claim 1 comprising the further steps of recovering said ceramic particles from said immiscible liquid and calcining said recovered particles to form a ceramic powder.

5. The method of claim 1 wherein said anhydrous alkanol sol is contacted with said immiscible liquid by introducing droplets of said sol to a continuous phase of said immiscible liquid.

6. The method of claim 5 wherein said droplets of sol are of colloidal size.

7. The method of claim 5 wherein said immiscible liquid is a hydrophilic liquid containing water and said sol is hydrophobic, whereby such spheroidizing step and hydrolysis step are effected simultaneously.

8. The method of claim 7 wherein said immiscible liquid is a mixture comprising acetonitrile, along with toluene, isopropanol, ethanol and water.

9. The method of claim 8 wherein said immiscible liquid contains up to 5 wt. % of water.

10. The method of claim 1 wherein said ceramic precursor is an alkoxide.

11. The method of claim 10 wherein said ceramic precursor concentration ranges from an alkoxide concentration of about 1 wt. % to about 80 wt. % of said sol.

12. The method of claim 4 wherein said at least one ceramic precursor comprises a mixture of aluminum-tri-sec-butoxide and zirconium n-butoxide, thereby to produce transformation toughened alumina ceramic particles.

13. The method of claim 3 wherein said sol is prepared by dispersing particles of at least one ceramic oxide precursor of colloidal particle size in a alkanol solvent.

14. The method of claim 13 wherein said alkanol has a concentration of from about 20 wt. % to about 99 wt. % of said sol.

15. The method of claim 12 wherein said alkanol solvent further comprises an organic hydrocarbon solvent to render the solvent highly hydrophobic.

16. The method of claim 15 wherein said alkanol solvent comprises isobutanol and toluene.

17. The method of claim 15 wherein said hydrocarbon solvent concentration is from about 12 wt. % to about 40 wt % of said sol.